CN108872283A - Using the method for wavelength dispersion X-ray fluorescence spectrometer measurement plant sample - Google Patents
Using the method for wavelength dispersion X-ray fluorescence spectrometer measurement plant sample Download PDFInfo
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- CN108872283A CN108872283A CN201811054020.1A CN201811054020A CN108872283A CN 108872283 A CN108872283 A CN 108872283A CN 201811054020 A CN201811054020 A CN 201811054020A CN 108872283 A CN108872283 A CN 108872283A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
Abstract
The invention discloses a kind of methods using wavelength dispersion X-ray fluorescence spectrometer measurement plant sample, by the selection of standard sample, the determination of measuring condition, prepare standard sample, the foundation of standard curve, the verifying of analysis method, monitoring sample：With prepare daily plant sample to be tested, measure the chemical content of each normal microelement in frequently seen plants sample.The method of present invention application Wavelength Dispersive-X-Ray fluorescence method analysis, reflect Plant Tolerance type, upgrowth situation, nutritive value and disease resistance trait and habitat characteristics etc., the drawbacks such as overcome traditional chemical routes time-consuming, is cumbersome, has the characteristics that accurate, convenient, economic, easy-operating, the research of botanizing or the plant nutrient generaI investigation etc. of suitable region large area.
Description
Technical field
The present invention relates to technical field of analysis and detection, in particular to a kind of application Wavelength Dispersive X-Ray Fluorescence Analysis to measure
The elements such as Cl, P, S, Sr, Rb, Pb, Br, Zn, Cu, Ni, Fe, Mn, Ti, Ba, Ca, K, Si, Al, Mg and Na in frequently seen plants sample
Method.
Background technique
In the analysis of traditional plant microelement, calcium and magnesium use volumetric method, and silicon uses gravimetric method, and aluminium uses aluminon colorimetric
Method, iron is using adjacent coffee sieve leaching colorimetric method and atomic absorption spectrophotometry, and manganese is using Gao Lin acid potassium colorimetric method and Atomic absorption point
Light photometry, copper and zinc use atomic absorption spectrophotometry.But these methods, when measuring element contents, often
All be that element is measured one by one, not only step is various, time-consuming more, and need using it is largely irritating to human body, to ring
There is the chemical reagent of pollution in border.Currently, the instruments such as atomic absorption method, inductively coupled plasma atomic emission spectrometry also by with
In micro elements by plants assay, but the sample pretreatment process of these methods is all to dissolve plant sample with chemicals,
The required sample preparation time is longer, is unfavorable for environmental monitoring and the quick progress of quality control process.
Summary of the invention
In view of above-mentioned, the purpose of the present invention is to provide a kind of application wavelength dispersion X-ray fluorescence spectrometers to measure plant
The method of sample, in particular to wavelength dispersion X-ray fluorescence spectrometer analyze measurement plant sample in Cl, P, S, Sr, Rb,
The method of the normal microelement such as Pb, Br, Zn, Cu, Ni, Fe, Mn, Ti, Ba, Ca, K, Si, Al, Mg and Na.
The purpose of the present invention is be achieved through the following technical solutions：
A method of plant sample being measured using wavelength dispersion X-ray fluorescence spectrometer, step is：
Step 1, the selection of standard sample：Biotic component series national standard reference substance is had chosen, is built as standard sample
Day-mark directrix curve,
Step 2, the determination of measuring condition：In conjunction with the actual disposition situation of Dutch Panaco PW4400 type Fluorescence Spectrometer, counting
The CONDITIONS IN INELASTIC ELECTRON of each analytical element in plant sample is had chosen in calculation machine：Analysis spectral line KA, LA；Collimator 150-
700mm;Detector is gas detector or scintillation detector or double detector；Voltage 30-60kV；Electric current 60-120mA；Crystal
23.25-144.83 ° of angle, it is arranged and optimizes channel measurement condition；
Step 3 prepares standard sample：The powder pressing method sample preparation for selecting boric acid fringing rebasing, weighs 4.00 gram particle degree in the balance
It less than the standard sample powder of 80 mesh, is put into sampling die, under the conditions of 32 tons of pressure, dwell time are 30s, is pressed
Internal diameter is made, and to be that 32 millimeters of disk is put into be measured in drier；
Step 4, the foundation of standard curve：The all higher standard substance GSB14 (seaweed) of each element content is chosen to scan one by one simultaneously
Indicate the peak value of each element, meanwhile, base is carried out using internal standard method, empirical coefficient method, theory Alpha Y-factor method Y and FP method are comprehensive
Body amendment establishes standard curve to deduct background and interference when the measurement of each element；
Step 5：The verifying of analysis method：The standard sample GSV1 bush branch and leaf for not participating in curve foundation is come as unknown sample
Measurement, it is known that, can evaluate each element determination precision due to constituent content in standard substance；Plant based on this method measurement
Owner's dimension cellulose content precision basically reaches the requirement of region plant elements generaI investigation, and the error of Main elements is within ± 5%, trace
The error of secondary element is within ± 25%；
Step 6 monitors sample：Drift is carried out to determination of plant method using monitoring standard specimen to correct, and is selected from calibration sample
As sample is checked, fluorescence analysis value and chemical score should coincide preferably one or several standard samples, every time before analysis
First measure this sample, the difference of measured value and standard value is in the margin of tolerance allowed；.
Step 7 prepares daily plant sample to be tested：The powder pressing method sample preparation for selecting boric acid fringing rebasing.Weigh 4 g
Granularity places it in less than 80 mesh powders and dries and be put into sampling die at 80 DEG C, under the pressure of 32 t, pressure maintaining
Time be 30 s under conditions of, be pressed into sample internal diameter be 32 mm print be put into it is to be measured in drier.
Step 8, examination with computer：According to the standard curve established, can find out Cl, P in sample to be tested, S, Sr, Rb,
The chemical content of 20 kinds of elements such as Pb, Br, Zn, Cu, Ni, Fe, Mn, Ti, Ba, Ca, K, Si, Al, Mg and Na.
Advantages of the present invention and the beneficial effect of generation are：
In view of the foregoing, the present invention is based on common Wavelength dispersion type x ray Fluorescence Spectrometer to establish frequently seen plants sample
The measuring method of the elements such as middle Cl, P, S, Sr, Rb, Pb, Br, Zn, Cu, Ni, Fe, Mn, Ti, Ba, Ca, K, Si, Al, Mg and Na.
In this invention, the pre-treatment of plant sample only needs to carry out being ground to 80 mesh to sample hereinafter, and utilizing powder pressing method pressure
Type is made, not only the required processing time is shorter, and the use of various chemical reagent is avoided during the pre-treatment of sample.
This method is relatively simple quickly, safety economy, while the drawbacks such as overcoming traditional chemical routes time-consuming, is cumbersome.Using X
Fluorescence spectrum method for measuring plant Major And Minor Elements content results can reflect Plant Tolerance type, upgrowth situation, nutritive value and disease-resistant
Character and habitat characteristics etc. can be applied to plant nutrient ingredient assessment, restore ecology, vegetation prospecting, soil and plant
In the fields such as heavy metal monitoring, it is especially suitable for the botanizing of region large area or grinding for plant nutrient generaI investigation etc.
Study carefully.
Detailed description of the invention
Fig. 1 is Cl element working curve in plant sample.
Fig. 2 is P element working curve in plant sample.
Fig. 3 is S element working curve in plant sample.
Fig. 4 is Sr element working curve in plant sample.
Fig. 5 is Rb element working curve in plant sample.
Fig. 6 is Pb element working curve in plant sample.
Fig. 7 is Br element working curve in plant sample.
Fig. 8 is Zn element working curve in plant sample.
Fig. 9 is Cu element working curve in plant sample.
Figure 10 is Ni element working curve in plant sample.
Figure 11 is Fe element working curve in plant sample.
Figure 12 is Mn element working curve in plant sample.
Figure 13 is Ti element working curve in plant sample.
Figure 14 is Ba element working curve in plant sample.
Figure 15 is Ca element working curve in plant sample.
Figure 16 is K element working curve in plant sample.
Figure 17 is Si element working curve in plant sample.
Figure 18 is Al element working curve in plant sample.
Figure 19 is Mg element working curve in plant sample.
Figure 20 is Na element working curve in plant sample.
Specific embodiment
With reference to the accompanying drawing, technical solution of the present invention is further described again：
A method of plant sample being measured using wavelength dispersion X-ray fluorescence spectrometer, step is：
Step 1, the selection of standard sample：Biotic component series national standard reference substance is had chosen as standard sample to build
Day-mark directrix curve, is shown in Table 1：
The national Certification of Biological Reference Materials of table 1
The biology of selection, chemical component, physical structure various aspects can be consistent with frequently seen plants sample, reduce structure
Effect and with granularity effect bring deviation, have sufficiently wide content range and concentration gradients appropriate, biology substantially
The content range for covering plant sample each element meets the needs of micro elements by plants assay, is shown in Table 2；
The content range of the national Certification of Biological Reference Materials of table 2
Note：Element unit with * is %, and the element unit without * is ug/g.
Step 2, the determination of measuring condition：In conjunction with the actual disposition situation of Dutch Panaco PW4400 type Fluorescence Spectrometer, counting
The CONDITIONS IN INELASTIC ELECTRON of each analytical element in plant sample is had chosen in calculation machine：Analysis spectral line KA, LA；Collimator 150-
700mm;Detector is gas detector or scintillation detector or double detector；Voltage 30-60kV；Electric current 60-120mA；Crystal
23.25-144.83 ° of angle, it is arranged and optimizes channel measurement condition, be shown in Table 3：
The measuring condition of the analysis measurement element of table 3
Step 3 prepares standard sample：The powder pressing method sample preparation for selecting boric acid fringing rebasing, weighs 4.00 gram particle degree in the balance
It less than the standard sample powder of 80 mesh, is put into sampling die, under the conditions of 32 tons of pressure, dwell time are 30s, is pressed
Internal diameter is made, and to be that 32 millimeters of disk is put into be measured in drier；
Step 4, the foundation of standard curve：The all higher standard substance GSB14 (seaweed) of each element content is chosen to scan one by one simultaneously
Indicate the peak value of each element, meanwhile, base is carried out using internal standard method, empirical coefficient method, theory Alpha Y-factor method Y and FP method are comprehensive
Body amendment improves the accuracy and precision of test result to deduct background and interference when the measurement of each element.With standard sample
The content of product element（Standard value）For abscissa, working curve is drawn as ordinate using the element count rate measured, passes through spectral line
Intensity and the explicit function form containing secondary element, establish standard curve；
Step 5：The verifying of analysis method：The standard sample GSV1 of curve foundation will not be participated in（Bush branch and leaf）As unknown sample
Product measure, due to constituent content in standard substance it is known that each element determination precision can be evaluated.By observed strength and theory
Intensity compares, and finds out the sensitivity coefficient of the element, when surveying unknown sample, the fluorescent X-ray intensity of sample is first measured, according to reality
It surveys intensity and sensitivity coefficient sets initial concentration value, then theoretical intensity is calculated by the concentration value.Intensity will be measured and theory is strong
Degree compares, and so that the two is reached a certain predetermined accuracy, otherwise to correct again, opposite to mark when being intended to sample content greater than 1%
Quasi- deviation is smaller than 1%.As can be seen from Table 4, national standard METHOD FOR CONTINUOUS DETERMINATION calculates, and compared with standard value, standard value and survey
Magnitude is close, and the plant Major And Minor Elements of this method measurement basically reach the requirement of region plant elements generaI investigation containing accuracy of measurement, main
The error of secondary element is within ± 5%, and the error of trace element is within ± 25%；
The standard value and measured value of 4 standard substance GSV1 of table
Note：Band*The unit of element is %, without*The unit of element is μ g/g.
Step 6, sets instrument, and the present invention uses sequential Wavelength dispersion type x ray Fluorescence Spectrometer, model：Axios
Advanced, manufacturer：Panaco instrument, the place of production：Holland；Monitor sample：Using monitoring standard specimen to determination of plant method into
Row drift is corrected, and selects from calibration sample one or several standard samples as checking sample, fluorescence analysis value with
Chemical score should coincide preferably, first measure this sample before analysis every time, the difference of measured value and standard value is in the tolerance model allowed
It encloses, then instrument can be directly used for routine analysis；
Step 7 prepares daily plant sample to be tested：The powder pressing method sample preparation for selecting boric acid fringing rebasing.Weigh 4 g granularities
It less than 80 mesh powders, places it in and dries and be put into sampling die at 80 DEG C, under the pressure of 32 t, the dwell time
Under conditions of 30 s, be pressed into sample internal diameter be 32 mm print be put into it is to be measured in drier；
Step 8, examination with computer：According to the standard curve established, can find out Cl, P in sample to be tested, S, Sr, Rb, Pb,
The chemical content of 20 kinds of elements such as Br, Zn, Cu, Ni, Fe, Mn, Ti, Ba, Ca, K, Si, Al, Mg and Na.
Claims (1)
1. a kind of method using wavelength dispersion X-ray fluorescence spectrometer measurement plant sample, step are：
Step 1, the selection of standard sample：Biotic component series national standard reference substance is had chosen, is built as standard sample
Day-mark directrix curve；
Step 2, the determination of measuring condition：In conjunction with the actual disposition situation of Dutch Panaco PW4400 type Fluorescence Spectrometer, counting
The CONDITIONS IN INELASTIC ELECTRON of each analytical element in plant sample is had chosen in calculation machine：Analysis spectral line KA, LA；Collimator 150-
700mm;Detector is gas detector or scintillation detector or double detector；Voltage 30-60kV；Electric current 60-120mA；Crystal
23.25-144.83 ° of angle, it is arranged and optimizes channel measurement condition；
Step 3 prepares standard sample：The powder pressing method sample preparation for selecting boric acid fringing rebasing, weighs 4.00 gram particle degree in the balance
It less than the standard sample powder of 80 mesh, is put into sampling die, under the conditions of 32 tons of pressure, dwell time are 30s, is pressed
Internal diameter is made, and to be that 32 millimeters of disk is put into be measured in drier；
Step 4, the foundation of standard curve：The all higher standard substance GSB14 (seaweed) of each element content is chosen to scan one by one simultaneously
Indicate the peak value of each element, meanwhile, base is carried out using internal standard method, empirical coefficient method, theory Alpha Y-factor method Y and FP method are comprehensive
Body amendment establishes standard curve to deduct background and interference when the measurement of each element；
Step 5：The verifying of analysis method：The standard sample GSV1 bush branch and leaf for not participating in curve foundation is come as unknown sample
Measurement, it is known that, can evaluate each element determination precision due to constituent content in standard substance；Plant based on this method measurement
Owner's dimension cellulose content precision basically reaches the requirement of region plant elements generaI investigation, and the error of Main elements is within ± 5%, trace
The error of secondary element is within ± 25%；
Step 6 monitors sample：Drift is carried out to determination of plant method using monitoring standard specimen to correct, and is selected from calibration sample
As sample is checked, fluorescence analysis value and chemical score should coincide preferably one or several standard samples, every time before analysis
First measure this sample, the difference of measured value and standard value is in the margin of tolerance allowed；
Step 7 prepares daily plant sample to be tested：The powder pressing method sample preparation for selecting boric acid fringing rebasing；
4 g granularities are weighed less than 80 mesh powders, places it in and dries and be put into sampling die at 80 DEG C, in 32 t
Pressure under, the dwell time be 30 s under conditions of, be pressed into sample internal diameter be 32 mm print be put into it is to be measured in drier；
Step 8, examination with computer：According to the standard curve established, can find out Cl, P in sample to be tested, S, Sr, Rb, Pb,
The chemical content of 20 kinds of elements such as Br, Zn, Cu, Ni, Fe, Mn, Ti, Ba, Ca, K, Si, Al, Mg and Na.
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| CN112697829A (en) * | 2020-11-18 | 2021-04-23 | 中国地质调查局西安地质调查中心(西北地质科技创新中心) | Method for measuring various elements in atmospheric particulates by taking actual sample as standard sample |
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Application publication date: 20181123 |